A simple, non-toxic, low-priced, and reproducible manipulation, which meets the standards of green chemistry, is introduced for the synthesis of ZnS x Se 1−x nanofibers. ZnS x Se 1−x nanofibers have been prepared in the entire composition range from ZnSe to ZnS by using a low-cost wet-chemical method. The effects of polymer (PVB) concentrations, reactant IJS/Se) concentrations and reaction conditions (applied voltage, viscosity, and work distance) have been investigated. We have demonstrated that wurtzite ZnS x Se 1−x showing a fiber-like morphology can be kinetically stabilized in the presence of an electrospinning system.One-dimensional (1D) semiconductor nanomaterials have received much attention for their unique electronic, optical, physical and chemical properties, and potential applications in optoelectronic devices, photonics, energy conversion, catalysis and biosensors. 1-3 Amid the group II-VI semiconductors, ZnSSe, as a direct band gap material with a bulk band gap of 2.70-3.5 eV, is considered as a good candidate for light-emitting devices and other optoelectronic devices. 4,5 Band gaps are one of the most significant factors in considering semiconductor materials for optoelectronic applications since they resolve the spectral characteristics of absorption and emission processes. Nanofibers open a new sight of band gaps through alloying with nearly assertive compositions. 6-8 ZnSe (bulk band gap 2.7 eV) and ZnS (bulk band gap 3.6 eV) are wide band gap semiconductor materials. These wide band gap semiconductors are also appealing hosts for the formation of doped nanomaterials. 9,10 For these reasons, synthesis of high-quality ZnSe and ZnS nanomaterials is still an attractive topic. [10][11][12][13][14][15][16] An important region in nanotechnology is the fabrication of composite structures containing different semiconductor nanocrystals. In semiconductor nanomaterials, band gap energy can easily be handled by slight tuning of their composition and size. Surface morphology also plays an important function in determining the properties of the system, especially on the nanoscale because of their large surface-tovolume ratio. Concomitant control of the morphology and structure of semiconductor nanomaterials provides chances to tune and research their optical properties. The properties of materials change dramatically with size and composition, which comprises thermodynamic stability. Also, structural transformations have been demonstrated to occur in nanoscale materials at lower temperatures. 17